Elastomer and process of producing same



I 3,055,819 Patented Sept. 25-, 1962 3,055,819 ELASTOMER AND PROESS F PRQDUCENG SAME Nathan W. Davis,3474 s. 22m St, Salt Lake City, Utah No Drawing. Briginal application Aug. 15, 1956, Ser. No. 604,085. Divided and this application Sept. 21, 1959, Ser. No. 846,527

2 Claims. (Cl. 204-162) 'more of these fractions to obtain an insecticidal composition.

It is a still further object of this invention to use one or "more of these fractions in compounding a paint composition.

A still further object of this invention is to use one of these distilled fractions in producing an elastomeric product.

Gilsonite is a black, brittle, lustrous mineral consisting of hydrocarbons, chiefly foundin the Southwestern section of the United States, principally in Utah and Colorado.

Destructive Distillation of Gilsonite In a steel still directly heated by means of electric resistance units is placed 50 pounds of Gilsonite, M.P. 320350 F. This still is connected to a water cooled condenser and the following fractions obtained at the temperatureindicated. For the purpose of further refer- :ence in this specification, these fractions have been give 'the following numbers.

Table of Gilsonite distillates using a 320 F. melt point Gilsonite. The following distillates are obtainable.

Specific Temperature, F. No. Color Gravity at 70 F.

clear 0.61 brownisl1 0. 73 clear slight re 1. 72 clear 1. 71

do 0.053 brownish black. 1. 31 clear 0.63 do 0.93 -do 1.12 reddish brown 1.19 385 to 397 do 2.11 390 to 393.- 12 clear.. 0. 74 13 do 0.87 14 do 0.89 15 slightly brown elea 0.79 16 reddish b 0.52 17 brown 0.90 18 clear 0. 67 19 brown 2. 69 20 clear 0.054 21 clear brown 0. 003 22 row-11.. 0. 94 23 clear 0.0041 24 clear reddish 0.005 25 brownish red 0.95 26 clean. 0.17 27 d0 0.19 28 brown. 1.03 29 0 0.039 30 brownish e1ear 0.73 31 clear.... 0.92 32 do 0.53 33 do 0.72 34 brow-n. 2.007 35 do 2.09

36 gray black dust, when cool, re-

maining in retort. Weight 120 grams to cu. inch.

More fractions are obtainable but they are not part of this invention.

EXAMPLE 1 A carbon silicate acid is obtained from the 16 fraction by treating as follows:

In a retort that will stand 600 pounds pressure, place-- 1 gal. distillate, fraction 16 12 oz. xylene (dimethylbenzene) 2 oz. triethanolamine (trihydroxytriethylamine) 6 oz. silicon mix (finely ground silicon dioxide 100 mesh) Heat to 250 F. maintaining a pressure of 30 pounds per square inch with continual agitation for one hour.

The retort is then allowed to cool, maintaining the agitation, and when cool, 1 gallon of distilled water is added. This is then distilled and three fractions taken at 230-240 F., 2602'70 F. and 310-315 F., using a water cooled condenser. The last fraction, that is, the one boiling at 310-315 F. is a fluid brownish liquid having a specific gravity of .24 at 70 F., and is then diluted with mineral spirits solvent in the ratio of 1 part distillate to parts solvent. The following solvents have also proven satisfactory; Stoddart Solvents manufactured by the Standard Oil Company and turpentine. This material has the following formula This is referred to in this application as Z It is a hydrocarbon silicon penetrating oil, a silicon carbonate or carboxy acetic acid.

Similar destructive distillation of coal or crude oil may be run and used in place of the 16th fraction from the destructive distillation of Gilsonite, after the addition of xylene triethanolamine and the silica and distilled, the fraction boiling at 260 F. for crude oil and 310 F. for coal can be used after dilution with mineral spirits.

A product is similarly obtained by treating the fraction as follows:

Mix in a heated retort with agitation- 1 gal. of #6 fraction (an oily brown, black material having a specific gravity of 1.31 .at 70 F.) v

7 oz. triethanolamine (trihydroxytriethylamine) 1 lb. silicon mix (finely ground silicon dioxide mesh) 20 oz. xylene (dimethylbenzene) .This material has the following formula:

4H 4CO OH (2Si O2H O EXAMPLE II.-PAINT A black colloidal non-toxic paint for waterproofing and rust-proofing metal, wood, concrete etc., which is resistant to heat, acid and alkali and moisture can be applied by brushing, spraying or dipping is prepared as follows:

Mix and heat in an open vessel 20 gal. petroleum solvent, such as mineral spirits or xylene 10 gal. boiled linseed oil 10 gal. turpentine, wood distilled or gum spirits of turpentine After heating to 100 F. slowly add lbs. pulverized -200 mesh Gilsonite, a pigment melting at 320-35 0 F. This mixture is then heated to 150 F., then slowly add 4 3 gals. of varnish (PT 358 National Lead Company) 1 gal. Petronate" 8 or 9 Sonneborn Sons Inc., New York, Wetting agent.

2 qts. of a mixture of 1 part lead, 1 part cobalt and 2 parts manganese drier 1 pt. of the penetrating oil not diluted, obtained as outlined above (Z16) This mixture is heated until the mixture reaches 200 F., continuously mixing for 15 minutes and then allowed to cool. It is drawn off and sealed in containers. This produces approximately 5 5 gals. of paint.

EXAMPLE III.ALUMINUM PAINT An aluminum paint, slightly toxic, which is resistant to heat, acid and alkali, as well as moisture, can be applied by spraying, brushing or dipping, is prepared as follows:

Mix in an open agitator- 12 gal. boiled linseed oil gal. petroleum solvent, such as mineral spirits or xylene 6 gal. paint prepared as in Example II 10 gal. 50-50 coal resin and petroleum solvent 50% ordinary coal resin 50% mineral spirits 3 gal. #30 aluminum pigment ground in oil 2 qts. Petr-onate 8 or 9 (wetting agent) (manufactured by Sonneborn Sons Inc. of New York) 2 qts. mixed drier (1 part lead, 1 part cobalt, 2 parts manganese) 1 pt. carbon silicate acid prepared as set forth above in Example I (Z16) Mix thoroughly until all of the aluminum pigment is suspended, then draw off and seal in containers.

EXAMPLE IV.-INSECTICIDES The following composition is prepared by mixing in an ordinary agitator:

10 lbs. wheat bran (vehicle) 1 pt. corn syrup (bait) 2 lbs. Gilsonite Z6 (poison) 2 oz. arsenic trioxide (optional) (poison) 2 oz. benzaldehyde (attractant) This insecticide is especially effective on earwigs, cockroaches and silver fish.

EXAMPLE V.-INSECTICIDES The following composition is prepared by mixing in an ordinary agitator.

Mix together with continuous agitation:

3 gal. kerosene (solvents) 2 gal. turpentine (solvents) 2 oz. oil of Pennyroyal (an essential oil) (attractant) 4 oz. creosol dip (poison) 6 oz. carbon-silicate acid Z6 prepared according to Example I given above before dilution with mineral spirits (poison) 1% oz. chlordane (octa-ohlor-hexahydro-methanoindene) (poison) 3 oz. odormask M, D, or H, Polok and Schwars Inc. of

New York This is particularly effective for termites, ants, spiders and related insects.

EXAMPLE VI.ELASTOMER This process is adapted to the use of any paraflinic hydrocarbon, such as Gilsonite, elaterite (commonly known as Wurtzalite). Bituminous coal may also be used. If bituminous coal is used as the basic material, the first step is slightly varied fiom the first step applicable when another hydrocarbon is used as the basic material.

Steps in the Process STEP NO. 1

A. For hydrocarbons other than bituminous coal: If a solid hydrocarbon other than coal is used as the base material, the hydrocarbon should be powdered. The first mass consists of 27 pounds or any multiple thereof, and based upon a 27 pound quantity, the materials are used in the following ratios:

20 pounds of Any parafiinic hydrocarbon, such as powdered Gilsonite, elaterite (Wurtzalite), hydrocarbons, etc. or asphalt of other semi-liquid hydrocarbon.

7 pounds of Raw linseed oil, or hydrogenated cottonseed oil or any other acid base vegetable oil.

27 pounds This mass as combined is mixed thoroughly until smooth, at normal room temperature.

B. If bituminous coal is used as the base material, the first step is as follows, using a mass of 27 pounds or any multiple thereof:

27 pounds These oils are processed by distillation by heating solids or semi-solid hydrocarbons to the temperatures F. as indicated.

This mass as combined is mixed thoroughly until smooth, at normal room temperature.

STEP NO. 2

Add to the foregoing base mass as compounded in Step No. 1, one pound of an oily wax. This wax should be added by mixing it with the base material described in Step No. 1.

STEP NO. 3

Add 1 /2 pounds of a sulfonated product obtained by treating cut No. 2 from the distillation of Gilsonite as described above, which boils within the range of 330 334 F. with sulfuric acid and then add 10% furfural and 5% oleic acid to of the sulfonated product. This is then distilled and a cut distilling at 340 F. to 590 F. The residue is an oily wax suitable for use in Step 2.

STEP NO. 4

Add one-half pound of furfural which will aid polymerization and also one pound of zinc sulphate which will act as an accelerator of polymerization.

STEP NO. 5

When all of the substances indicated in Steps Nos. 1, 2, 3 and 4 have been combined, regardless of which substance is first added to the mixed mass of Step No. 1, whether material described in Steps Nos. 2, 3 or 4, the aggregate of all of these substances should be mixed thoroughly for approximately one hour at ordinary room temperature, not less than 40 F. nor in excess of F.

STEP NO. 6

The aggregate so compounded and mixed is then subjected to slow heat. The temperature should he stepped up gradually until it reaches 200 F. within a period of two and one-half hours, during which time the compounded substances should be mixed at a moderate speed. The compounded substances should continue to be mixed at such speed for approximately 6 hours at 200 F. from the time when such temperature is first reached.

STEP NO. 7

The temperature is then gradually increased to 350 F. with an increase of vpressure .to 50 pounds, the mixing continuing during this increasein temperature. This mixing process at 50 pounds pressure and at 350 F. temperature continues for about 64 hours.

STEP NO. 8

The temperature is then slowly decreased to 250 F. over a period of about 3 hours, during which time the mixing process continues.

STEP NO. 9

Two pounds of water and one pound of potassium sulfate for a plasticizer, are then added to the mass while the mixing process continues.

STEP NO. 10

The temperature remains at 250 F. while the pressure is increased to 60 pounds by the addition of the water as indicated in Step No. 9. This pressure and this temperature are maintained for about 3 hours while the mixing continues.

STEP NO. 11

The pressure and temperature are then reduced slowly until pressure is entirely released and reduced to zero, and the temperature is reduced to 100 F., while mixing continues.

STEP NO. 12

At this stage 2 pounds of sulphur (which should be at least 90% pure, if possible) should be added to the mass, unless the base material is a high contained type asphalt in which event sulphur is not added. There should also be added at this stage of the processing pounds of calcium oxide. These ingredients should be mixed into the mass for about 8 hours at a temperature of about 100 F., in an open container under sunlight or ultraviolet rays or other light which produces the same general reaction as sunlight.

STEP NO. 13

The mixing process is then retarded until the mass becomes rubbery and appears somewhat dry. This period should normally occupy about 4 hours.

STEP N0. 14

The processed mass is then removed from the autoclave or other suitable mixing machine which has pressure and heating facilities, and then cured by sunlight or artificial light having similar reaction power. The length of this phase of the process depends upon intensity of light and humidity. Sufficient moisture must be in the atmosphere to facilitate the curing process.

STEP NO. 15

The cured mass is then ready for use. The material is also in condition for introduction of any rubber extenders or fillers, if desired, to give the elastomer a different degree of resiliency, or in order to reduce elasticity.

EXAMPLE VII.ORE REDUCTION PROCESS This process is adapted to a separation of complex mineral ores after the raw ore has been crushed and ground to the customary mesh common in conventional means of ore separation. The process is adaptable to all types of complex minerals including radioactive material, ferrous .and nonferrous minerals.

Steps in the Process STEP NO. 1

The complex ore as it comes from the ball mill or other grinding device at the required mesh is placed into an agitated heated tank for conditioning where the ore material is mixed with warm water to a specific gravity of 60. Sulfuric acid is then mixed with the material in an amount equal to 1% of the lime content of the ore material while in the process of raisin the temperature of the slurry to 200 F. Said temperature should not be obtained however until after completion .of the second STEP NO. 3

Now add hydrochloric acid in an amount equal to A of the sulfuric acid previously added. Continue to mix or agitate for thirty minutes or until the slurry reaches the temperature of 200 F., whichever occurs first.

STEP NO. 4

Now introduce sodium bicarbonate into tank No. 2 in an amount by weight equivalent to twice the number of pounds of sulfuric acid by weight which has been previously added, then empty tank No. 1 into tank No. 2

and slowly agitate.

STEP NO. 5

Then add potassium iodine in an amount equivalent of 2% of the sodium previously added.

STEP NO. 6

Then add and miX into the slurry aluminum nitrate in an amount equivalent of 1% of the potassium iodine previously used. The agitation is now discontinued and the material allowed to settle. A scum forms on the top which is skimmed off and introduced into a separate tank No. 3 containing the same amount of sodium sulfate as there was potassium iodine used previously. Here the scum or material skimmed ofi settles and the precipitant is drawn off into evaporating tanks. This is the radioactive material.

STEP NO. 7

If the ore headings contain carbon, use nitric acid in place of sulfuric acid in the preceding steps.

STEP NO. 8

The aforesaid steps permit the separation of various ores in the precipitant material contained in tank No. 2 or the soda tank as described in Step No. 4. The various ore particles are free and independent of each other and can be concentrated by conventional methods such as tabling or flotation.

Many minor changes could be made in the above process as described in this .application. All such changes come within the scope of this invention. The important feature is the introduction of the Z16 material and its faculty to penetrate through and cause separation at the microscopic seams or contact points between the various kinds of ore particles which are commonly found united together in most ore material.

What is claimed is:

l. A process for producing an elastomer which comprises, (1) mixing 20 parts of paraflin hydrocarbon and 7 parts of linseed oil, (2) adding 1 /2 parts of a Wax obtained by treating the distillate boiling approximately within the range of 330 to 334 F. from the destructive distillation of Gilsonite with sulfuric acid, adding furfural and oleic acid and distilling the same to obtain a Wax residue boiling between 340 F. to 590 F., (3) adding /2 part of furfural and 1 part of a polymerization promoter, (4) mixing at a temperature of 40 to F. for one hour, (5 slowly heating until the temperature reaches 200 F., (6) maintaining this temperature for six hours, (7) increasing the temperature to 350 F., maintaining a pressure of 50 lbs. for a period of 64 hrs., (8) slowly decreasing the temperature to 250 F. over a period of References Cited in the file of this patent three hours, (9) adding 2 partsof water and 1 part of UNITED STATES PATENTS potasslum sulfate and malntalning the pressure at 60 lbs. for a period of three hours, (10) reducing the tem- 255,139 Burr Mar. 21, 1882 perature to 100 F. and adding 2 parts of sulfur and 5 5 1,954,866 Eglofl Apr. 17, 1934 parts of calcium oxide and mixing the same for eight 1,972,944 Morrell Sept. 11, 1934 hours at a temperature of 100 F. with exposure to sun- 2,386,448 Dreisbach Oct. 9, 1945 light, and (11) the mass being then cured by extended exposure to sunlight. OTHER REFERENCES 2. An elastorn whi h i produced by the Process 10 Abraham: Asphalts and Allied Substances, 5th ediaccordmg to claw tion, vol. 1, 1945, 1. 253. 

1. A PROCESS FOR PRODUCING AN ELASTOMER WHICH COMPRISES, (1) MIXING 20 PARTS OF PARAFFIN HYDROCARBON AND 7 PARTS OF LINSEED OIL, (2) ADDING 11/2 PARTS OF A WAX OBTAINED BY TREATING THE DISTILLATE BOILING APPROXIMATELY WITHIN THE RANGE OF 330 TO 334*F. FROM THE DESTRUCTIVE DISTILLATION OF GILSONITE WITH SULFURIC ACID, ADDING FURFURAL AND OLEIC ACID AND DISTILLING THE SAME TO OBTAIN A WAX RESIDUE BOILING BETWEEN 340* F. TO 590* F., (3) ADDING 1/2 PART OF FURFURAL AND 1 PART OF A POLYMERIZATION PROMOTER, (4) MIXING AT A TEMPERATURE OF 40 TO 120* F. FOR ONE HOUR, (5) SLOWLY HEATING UNTIL THE TEMPERATURE REACHES 200*F., (6) MAINTAINING THIS TEMEPERATURE FOR SIX HOURS, (7) INCREASING THE TEMPERATURE TO 350*F., MAINTAINING A PRESSURE OF 50 LBS. FOR A PERIOD OF 64 HRS., (8) SLOWLY DECREASING THE TEMPERATURE TO 250*F. OVER A PERIOD OF THREE HOURS, (9) ADDING 2 PARTS OF WATER AND 1 PART OF POTASSIUM SULFATE AND MAINTAINING THE PRESSURE AT 60 LBS. FOR A PERIOD OF THREE HOURS, (10) REDUCING THE TEMPERATURE TO 100*F. AND ADDING 2 PARTS OF SULFUR AND 5 PARTS OF CALCIUM OXIDE AND MIXING THE SAME FOR EIGHT HOURS AT A TEMPERATURE OF 100*F. WITH EXPOSURE TO SUNLIGHT, AND (11) THE MASS BEING THEN CURED BY EXTENDED EXPOSURE TO SUNLIGHT. 